CN101982471B - Technological process for extracting aucubin from fruits of eucommia ulmoides oliver - Google Patents
Technological process for extracting aucubin from fruits of eucommia ulmoides oliver Download PDFInfo
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- CN101982471B CN101982471B CN 201010297478 CN201010297478A CN101982471B CN 101982471 B CN101982471 B CN 101982471B CN 201010297478 CN201010297478 CN 201010297478 CN 201010297478 A CN201010297478 A CN 201010297478A CN 101982471 B CN101982471 B CN 101982471B
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Abstract
The invention relates to a technological process for extracting aucubin from fruits of eucommia ulmoides oliver, which comprises the following steps: cutting the fruits of the eucommia ulmoides oliver into pieces, extracting with water or ethanol solution as an extraction solvent, and purifying the obtained extracting solution with macroporous resin to obtain the aucubin the purity of which is more than 50%. The technological process has the advantages of low toxicity, safety, short process time, no environmental pollution, simple and convenient operation, easy industrialization enlargement, high yield and good purity of the product, thus meeting various needs for development of drugs taking the fruits of the eucommia ulmoides oliver as main raw materials.
Description
[technical field]
The present invention relates to the extraction and separation method of effective ingredients in plant in the pharmaceutical industry, particularly a kind of processing method of from bark of eucommia fruit, extracting aucubin.
[background technology]
Aucubin (aucubin) belongs to iridoid glycosides, and molecular formula is C
15H
22O
9, molecular weight 346.331, CAS number is 479-98-1,181 ℃ of fusing points, soluble in water, ethanol and methyl alcohol are dissolved in chloroform, ether and sherwood oil hardly.This compound mainly is present in the plants such as bark of eucommia Eucommia ulmoides Oliver, Cornaceae plant peach jaurel Aucubachinensis Benth., the front Plantago asiatica L. of Plantaginaceae plant car, be one of medium-height grass the effective elements of the medicines such as the bark of eucommia, psyllium, glutinous rehmannia, have numerous pharmacologically actives such as liver detoxification, anti-inflammatory, anti-oxidant, anti-ageing, osteoporosis and trophic nerve unit cell.The aucubin structural formula is as follows:
The bark of eucommia really belongs to the fruit of single kind of plant bark of eucommia Eucommia ulmoides Oliver for the Eucommiaceae bark of eucommia, be China's endemic plant, aboundresources.The medicinal beginning of Cortex Eucommiae is stated from Shennong's Herbal, classifies as top gradely, has invigorating the liver and kidney, strengthening the bones and muscles, antiabortive effect, can be used for treating the diseases such as spinal column ache, impotence, frequent micturition, dribbling urination, rheumatic arthralgia, threatened abortion, habitual abortion.The research emphasis of this plant is the pharmaceutical use of lignanoid in Cortex Eucommiae and the Folium Eucommiae, chlorogenic acid compound at present, and the bark of eucommia is really utilized seldom, has caused the wasting of resources.Retrieve according to the applicant, existing bark of eucommia fruit patent is all relevant with eucommia ulmoides seed oil, and other has the related journals paper of one piece of extraction aucubin from bark of eucommia fruit, and (Peng Mijun prints big-and-middle, Liu Liping, Deng. the preparation of rhinanthin in the seed of bark of eucommia dregs of rice. fine chemistry industry, 2007,24 (3): 243-247), the thesis the preparation of microwave method and reversed-phase preparative chromatography technology, this process costs is very high, and preparation process is loaded down with trivial details, is unfavorable for large production operation.
[summary of the invention]
The objective of the invention is in order to overcome the deficiencies in the prior art, and a kind of new process that extracts aucubin from bark of eucommia fruit is provided, the method can obtain the higher aucubin of purity, and is conducive to large production operation.
The present invention is that to address the above problem the scheme that adopts be a kind of new process that extracts aucubin from bark of eucommia fruit of design.It may further comprise the steps:
1. the bark of eucommia of drying is really shredded, water or alcohol concn are that 0%～70% the aqueous solution is undertaken filtering after cold soaking or the refluxing extraction by 1: 3～1: 10 weightmeasurement ratio of feed liquid to bark of eucommia fruit, get filtrate;
2. concentrated filtrate gets the feed liquid weightmeasurement ratio and is 1: 1～1: 3 concentrated solution;
3. first with the concentrated solution absorption with macroporous adsorbent resin, wherein macroporous adsorbent resin is 1～5: 1 with the weight ratio of the bark of eucommia fruit medicinal material of drying; Then water or alcohol concn are that 0%～30% aqueous solution wash-out is removed impurity, use the aqueous solution wash-out of 20～90% ethanol again, collect elutriant;
4. elutriant is concentrated rear dry, namely get bark of eucommia berry extract.
The invention has the beneficial effects as follows: the extraction, the separation purification method that the invention provides aucubin in the bark of eucommia fruit.This method only namely obtains purity greater than 50% aucubin by the purifying process of a step macroporous adsorbent resin, and a water and ethanol are as solvent in the preparation process, and non-environmental-pollution can reuse for several times after the used macroporous adsorbent resin regeneration, and cost is low.This technological operation is easy, is easy to realize that industrialization amplifies, and product yield is high, purity is good, can satisfy various take the bark of eucommia really as the needs of the drug development of main raw material.
[description of drawings]
Fig. 1 is for using the resulting aucubin HPLC of the inventive method collection of illustrative plates.
Be described in detail below in conjunction with embodiments of the invention.
[embodiment]
The present invention adopts following technical proposal:
The bark of eucommia of drying is really shredded, and water or the bark of eucommia is really undertaken filtering after cold soaking or the refluxing extraction by 1: 3～1: 10 weightmeasurement ratio of feed liquid less than 70% aqueous ethanolic solution gets filtrate;
Concentrated filtrate gets concentrated solution;
With concentrated solution with absorption with macroporous adsorbent resin after, successively water, aqueous ethanolic solution wash-out are collected elutriant;
Dry after elutriant is concentrated, namely get aucubin content and reach bark of eucommia berry extract more than 50%.
Above-mentioned preparation method 3. in the model of macroporous adsorbent resin be among NKA-9, S-8, D4020 or the D301R one or more, used macroporous adsorbent resin and the bark of eucommia really weight ratio of medicinal material are 1～5: 1.Concrete operations are first water or remove decon less than 30% ethanol aqueous wash, use the aqueous solution wash-out of 20～90% ethanol again, and the water that twice wash-out used or the consumption of aqueous ethanolic solution all are 2～8 times of column volumes.
Above-mentioned preparation method 4. described in drying means be drying means as known in the art, for example: spraying drying, drying under reduced pressure, microwave drying or lyophilize.
Embodiment 1
Get bark of eucommia fruit medicinal material 1kg, with chopper fruit is cut into 3～4 sections, add water 6L, soaked 3 hours, refluxing extraction 2 hours is filtered; The dregs of a decoction add water 5L again, refluxing extraction 2 hours, filter, the dregs of a decoction extract 1 time with same method again, merging filtrate, being concentrated into medicine liquid volume is 2: 1 with the quality of medicinal material ratio, be added to the NKA-9 type handled well (Tianjin Nankai with become Science and Technology Ltd.) macroporous adsorptive resins (the about 2.3L of resin bed volume, the weight ratio that is equivalent to resin and medicinal material is 1.5: 1) on, use first 3 times of water elutions to resin bed volume (3BV) extremely almost colourless, discard elutriant, use again 80% aqueous ethanolic solution wash-out, every 600ml collects a, collects 15 parts (being equivalent to approximately 4BV), detects, merge 6～13 parts of elutriants according to detected result, 60 ℃ of decompression recycling ethanols, spraying drying namely get bark of eucommia berry extract 47.2g, and aucubin content is 56.9% in the HPLC Detection and Extraction thing.
Embodiment 2
Get bark of eucommia fruit medicinal material 5kg, with chopper fruit is cut into 3～4 sections, add 50% aqueous ethanolic solution 30L, soaked 3 hours, refluxing extraction 2 hours is filtered; The dregs of a decoction add 50% aqueous ethanolic solution 25L again, refluxing extraction 2 hours, filter, the dregs of a decoction extract 1 time with same method again, merging filtrate, being concentrated into medicine liquid volume is 2: 1 with the quality of medicinal material ratio, be added to the S-8 type handled well (Tianjin Nankai with become Science and Technology Ltd.) macroporous adsorptive resins (the about 15L of resin bed volume, the weight ratio that is equivalent to resin and medicinal material is 5: 1) on, use first 3 times of water elutions to resin bed volume (3BV) extremely almost colourless, discard elutriant, use again 60% aqueous ethanolic solution wash-out, every 4000ml collects a, collects 15 parts (being equivalent to approximately 4BV), detects, merge 7～11 parts of elutriants according to detected result, 60 ℃ of decompression recycling ethanols, drying under reduced pressure namely get bark of eucommia berry extract 167.5g, and aucubin content is 68.1% in the HPLC Detection and Extraction thing.
Embodiment 3
Get bark of eucommia fruit medicinal material 10kg, with chopper fruit is cut into 3～4 sections, add 10% aqueous ethanolic solution 60L, soaked 3 hours, refluxing extraction 2 hours is filtered; The dregs of a decoction add water 50L again, refluxing extraction 2 hours, filter, the dregs of a decoction extract 1 time with same method again, merging filtrate, being concentrated into medicine liquid volume is 2: 1 with the quality of medicinal material ratio, be added to the D301R type handled well (Tianjin Nankai with become Science and Technology Ltd.) macroporous adsorptive resins (the about 36L of resin bed volume, the weight ratio that is equivalent to resin and medicinal material is 3: 1) on, use first 3 times of water elutions to resin bed volume (3BV) extremely almost colourless, discard elutriant, use again 50% aqueous ethanolic solution wash-out, every 8000ml collects a, collects 18 parts (being equivalent to approximately 4BV), detects, merge 5～10 parts of elutriants according to detected result, 60 ℃ of decompression recycling ethanols, spraying drying namely get bark of eucommia berry extract 432.8g, and aucubin content is 60.6% in the HPLC Detection and Extraction thing.
Claims (5)
1. processing method of extracting aucubin from bark of eucommia fruit may further comprise the steps:
1. the bark of eucommia of drying really being shredded, is that 0%～70% the aqueous solution is undertaken filtering after cold soaking or the refluxing extraction by 1: 3～1: 10 weightmeasurement ratio of feed liquid to bark of eucommia fruit with alcohol concn, gets filtrate;
2. concentrated filtrate gets the feed liquid weightmeasurement ratio and is 1: 1～1: 3 concentrated solution;
3. first with the concentrated solution absorption with macroporous adsorbent resin, wherein macroporous adsorbent resin is 1～5: 1 with the weight ratio of the bark of eucommia fruit medicinal material of drying; Then be that 0%～30% aqueous solution wash-out is removed impurity with alcohol concn, use again 20～90% aqueous ethanolic solution wash-out, collect elutriant;
4. elutriant is concentrated rear dry, namely get bark of eucommia berry extract.
2. the processing method of extracting aucubin from bark of eucommia fruit as claimed in claim 1 is characterized in that: the macroporous adsorbent resin that step is used described in 3. is among NKA-9, S-8 or the D4020 one or more.
3. the processing method of extracting aucubin from bark of eucommia fruit as claimed in claim 1 or 2 is characterized in that: step 3. in the consumption of the aqueous ethanolic solution used of twice wash-out all be 2～8 times of column volumes.
4. the processing method of extracting aucubin from bark of eucommia fruit as claimed in claim 3 is characterized in that: step is dry described in 4. to be spraying drying, drying under reduced pressure, microwave drying or lyophilize.
5. the processing method of extracting aucubin from bark of eucommia fruit as claimed in claim 3 is characterized in that: described step 4. in the gained bark of eucommia berry extract aucubin content reach more than 50%.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219814A (en) * | 2011-05-25 | 2011-10-19 | 河南大学 | Method for extracting aucubin from eucommia ulmoides oliver seed draff |
| CN102603828A (en) * | 2012-02-22 | 2012-07-25 | 李光锋 | Method for extracting aucubin from eucommia bark leaves |
| CN104666393A (en) * | 2014-07-09 | 2015-06-03 | 普正药业股份有限公司 | Anti-osteoporosis eucommia ulmoides sustained-release tablet and preparation method thereof |
| CN110236968A (en) * | 2019-07-03 | 2019-09-17 | 深圳市诗碧曼科技有限公司 | A kind of antibacterial mouthwash of anti-ageing healthcare and preparation method thereof |
| CN113045531A (en) * | 2021-03-31 | 2021-06-29 | 深圳市诗碧曼科技有限公司 | Method and device for extracting and synthesizing aucubin aglycone with high yield |
| CN113663003A (en) * | 2021-09-22 | 2021-11-19 | 中国药科大学 | Effective component group of Linum macrocarpum root as well as preparation method and application thereof |
| CN113980064B (en) * | 2021-11-02 | 2023-08-29 | 广东省科学院测试分析研究所(中国广州分析测试中心) | Preparation method and application of high-purity aucubin |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225095A (en) * | 2008-01-22 | 2008-07-23 | 西安交通大学 | Method for extracting aucubin from pedicularis plants |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225095A (en) * | 2008-01-22 | 2008-07-23 | 西安交通大学 | Method for extracting aucubin from pedicularis plants |
Non-Patent Citations (3)
| Title |
|---|
| 张永康等.超临界二氧化碳萃取杜仲果实中桃叶珊瑚苷工艺研究.《林产化学与工业》.2006,第26卷(第4期),第113-116页. * |
| 董娟娥等.大孔吸附树脂一次性分离杜仲叶中杜仲总苷和杜仲黄酮的研究.《农业工程学报》.2006,第22卷(第7期),第154-158页. * |
| 郭丽冰等.大孔吸附树脂对桃叶珊瑚苷分离效果的研究.《中药研究与信息》.2005,第7卷(第9期),第21-22页. * |
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